CN115838493B - Porous structure shielding wave-absorbing composite material and preparation method thereof - Google Patents
Porous structure shielding wave-absorbing composite material and preparation method thereof Download PDFInfo
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Abstract
The application discloses a porous structure shielding wave-absorbing composite material and a preparation method thereof, wherein the preparation method comprises the steps of preparing a non-compact carbon nano tube continuous network aggregate; adding mixed powder into the non-dense carbon nano tube continuous network aggregate, and rolling to obtain a film material; the mixed powder comprises a high molecular polymer, shielding wave-absorbing particles and foaming powder; and after one or more layers of membrane materials are combined together, placing the membrane materials in an environment with the temperature of more than 100 ℃ to enable the high polymer to be melted, and expanding and foaming the foaming powder to form hollow microspheres to obtain the porous structure shielding wave-absorbing composite material. The preparation method provided by the application is simple, easy to operate and low in cost, and the prepared porous structure shielding wave-absorbing composite material keeps the continuous network structure of the carbon nano tube, and has the advantages of light weight, thin thickness, wide adaptive frequency band, strong shielding effectiveness, good conductivity and the like.
Description
Technical Field
The application discloses a porous structure shielding wave-absorbing composite material and a preparation method thereof, and belongs to the technical field of composite materials.
Background
With the development of electronic and information technologies, electromagnetic waves penetrate into various aspects of daily life, and more particularly network safety and national defense safety are related, and electromagnetic shielding has important influences on daily life, human health, equipment operation, information safety, weaponry and the like.
Electromagnetic shielding is a measure in a certain region of space to attenuate the field strength caused by certain sources. The electromagnetic shielding material in the prior art can be copper, aluminum, steel and other metals or ferrite and the like.
From the above, the existing electromagnetic shielding material is mainly a single material, but the single material has the disadvantages of large mass, high cost, large thickness, insufficient shielding efficiency and the like, and is difficult to meet the requirement of high-performance electromagnetic shielding.
Disclosure of Invention
The application aims to provide a porous structure shielding wave-absorbing composite material and a preparation method thereof, which are used for solving the technical problems of large mass, high cost, large thickness and insufficient shielding effectiveness of a single electromagnetic shielding material in the prior art.
The first aspect of the application provides a preparation method of a porous structure shielding wave-absorbing composite material, which comprises the following steps:
preparing a non-dense carbon nano tube continuous network aggregate;
adding mixed powder into the non-dense carbon nanotube continuous network aggregate, and rolling to obtain a film material; the mixed powder comprises a high molecular polymer, shielding wave-absorbing particles and foaming powder;
and after one or more layers of membrane materials are combined together, placing the membrane materials in an environment with the temperature of more than 100 ℃ to enable the high polymer to melt, and expanding and foaming the foaming powder to form hollow microspheres to obtain the porous structure shielding wave-absorbing composite material.
Preferably, the volume of the high molecular polymer is more than 30% of the total volume of the mixed powder.
Preferably, the volume ratio of the high molecular polymer to the shielding wave-absorbing particles to the foaming powder is 1:1:1.
Preferably, the high molecular polymer is a thermoplastic or thermosetting resin material;
the material used for shielding the wave-absorbing particles is ferrite wave-absorbing material and micro powder wave-absorbing material;
the foaming powder is sodium bicarbonate foaming agent or sodium dodecyl sulfate.
Preferably, the rolling is performed after adding the mixed powder into the non-dense carbon nanotube continuous network aggregate, specifically including:
and uniformly adding mixed powder into the non-dense carbon nano tube continuous network aggregate in a physical deposition mode, and then rolling.
Preferably, after one or more layers of the film materials are combined together, they are placed in an environment with a temperature greater than 100 ℃, and specifically include:
after one or more layers of the membrane materials are combined together, limiting plates are arranged on the upper surface and the lower surface of the combined membrane materials;
and placing the combined membrane material provided with the limiting plates in an environment with the temperature of more than 100 ℃.
Preferably, the particle size of the high molecular polymer, the shielding wave-absorbing particles and the foaming powder in the mixed powder is micro-particle size or nano-particle size.
Preferably, the particle size of the high molecular polymer, the shielding wave-absorbing particles and the foaming powder in the mixed powder is smaller than 30 mu m.
The second aspect of the application provides a porous structure shielding wave-absorbing composite material prepared by the preparation method of the porous structure shielding wave-absorbing composite material.
Preferably, the thickness of the porous structure shielding wave-absorbing composite material is 2mm-4mm, and the density is 1.5g/cm 3 -2g/cm 3 。
Compared with the prior art, the porous structure shielding wave-absorbing composite material and the preparation method thereof have the following beneficial effects:
the preparation method provided by the application is simple, easy to operate and low in cost, and the prepared porous structure shielding wave-absorbing composite material keeps the continuous network structure of the carbon nano tube, and has the advantages of light weight, thin thickness, wide adaptive frequency band, strong shielding effectiveness, good conductivity and the like.
Drawings
FIG. 1 is a flow chart of a method for preparing a porous shielding wave-absorbing composite material according to an embodiment of the application;
fig. 2 is a graph showing electromagnetic shielding effect of a porous structure shielding wave-absorbing composite material according to an embodiment of the present application.
Detailed Description
In the following description, for purposes of explanation and not limitation, specific details are set forth such as the particular system architecture, techniques, etc., in order to provide a thorough understanding of the embodiments of the present application. It will be apparent, however, to one skilled in the art that the present application may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known systems, devices, circuits, and methods are omitted so as not to obscure the description of the present application with unnecessary detail.
The first aspect of the present application provides a method for preparing a porous shielding wave-absorbing composite material, the flow of which is shown in fig. 1, comprising:
step 1, preparing a non-dense carbon nano tube continuous network aggregate, which specifically comprises the following steps:
carbon-containing organic matters such as ethanol, methane and acetylene are used as carbon sources, are injected into a high-temperature furnace tube in a solid sublimation or liquid atomization mode, and move from a feed end to a discharge end along the axial direction of the furnace tube under the action of air flow taking hydrogen, argon and nitrogen as main carrier gases, in the process, the carbon-containing organic matters are subjected to high-temperature pyrolysis to form carbon atoms, in-situ chemical reaction is carried out under the action of a catalyst containing Fe and S (such as ferrocene and thiophene), carbon nano tubes are generated, and assembled into a macroscopic body of the carbon nano tubes under the action of carrier gas flow, and the macroscopic body of the carbon nano tubes is collected layer by layer at the discharge end of the furnace tube to form a non-compact continuous network aggregate of the carbon nano tubes.
The carbon nano tube in the embodiment of the application is a high-conductivity one-dimensional linear material with a larger length-diameter ratio. On one hand, the carbon nano tube material has very high length-diameter ratio, so that agglomeration is easy to occur, and the carbon nano tube material is difficult to uniformly disperse in a polymer; on the other hand, carbon nanotubes are difficult to form a continuous conductive network in a polymer, which results in poor electromagnetic shielding performance and influences the mechanical properties of the composite material. The carbon nano tube continuous network aggregate prepared by the method provided by the embodiment of the application is of a skeleton structure, and the problem of local agglomeration does not exist, so that the mixed powder is convenient to be added into the carbon nano tube continuous network aggregate in the follow-up process, and the finally prepared porous structure shielding wave-absorbing composite material is stable in performance. And the shielding wave-absorbing particles and the foaming powder are added into the carbon nano tube by utilizing the subsequent step 2, so that the carbon nano tube has better conductivity, electromagnetic shielding efficiency and stability.
Step 2, adding mixed powder into the non-dense carbon nanotube continuous network aggregate, and then rolling to obtain a membrane material; wherein the mixed powder comprises high molecular polymer, shielding wave-absorbing particles and foaming powder.
Wherein the particle size of the high molecular polymer, the shielding wave-absorbing particles and the foaming powder in the mixed powder is micron-sized particle size or nanometer-sized particle size. The particle sizes of the three materials can be the same or different, for example, the particle sizes of the high molecular polymer, the shielding wave-absorbing particles and the foaming powder are all smaller than 30 mu m, or the particle sizes of the high molecular polymer and the shielding wave-absorbing particles are all smaller than 25 mu m, and the particle size of the foaming powder is larger than 35 mu m.
In the embodiment of the application, the step 2 specifically comprises the following steps:
and step 21, uniformly or non-uniformly adding mixed powder into the non-dense carbon nano tube continuous network aggregate by a physical deposition mode.
The physical deposition mode in the embodiment of the application is specifically realized as follows: and (3) scattering the micron-sized or nano-sized mixed powder into the non-compact carbon nano tube continuous network aggregate by adopting an automatic or non-automatic vibrating screen powder scattering device.
In order to ensure that the prepared porous structure shielding wave-absorbing composite material has uniform performance, the embodiment of the application preferably utilizes an automatic vibrating screen powder scattering device to uniformly distribute mixed powder in the carbon nano tube continuous network aggregate.
In order to ensure that the relative positions of the shielding wave-absorbing particles and the foaming powder are unchanged, and thus ensure that the performance of each part of the prepared porous shielding wave-absorbing composite material is stable, the volume of the high polymer in the mixed powder in the embodiment of the application is more than 30%, such as 31%,33%,34%,50% and the like of the total volume of the mixed powder, wherein the high polymer is a thermoplastic or thermosetting resin material, and can be polyimide, epoxy resin, polyether-ether-ketone and the like. The thermoplastic or thermosetting resin material with the volume can enable the thermoplastic or thermosetting resin material to be melted and then fully cover all shielding wave-absorbing particles and foaming powder, uniformly bond hollow microspheres formed by the carbon nano tubes and the foaming powder and shielding wave-absorbing particles together, and ensure that the relative positions of all shielding wave-absorbing particles and the foaming powder in the carbon nano tube continuous network aggregate are fixed.
In the embodiment of the application, the material used for shielding the wave-absorbing particles can be ferrite wave-absorbing material, micro powder wave-absorbing material, polycrystalline ferromagnetic metal fiber, schiff base retinyl, and the like, and the ferrite wave-absorbing material has the advantages of strong absorption and wide frequency band, so the ferrite wave-absorbing material is preferably used, and the ferrite wave-absorbing material can be nickel zinc ferrite, manganese zinc ferrite, barium ferrite, and the like.
The foaming powder in the embodiment of the application is sodium bicarbonate foaming agent or sodium dodecyl sulfate. The hollow microsphere formed by the foaming powder not only can play a role in reducing weight, but also is beneficial to dielectric loss of electromagnetic waves and improves electromagnetic wave absorption capacity. The shielding effect can be greatly improved by the cooperation of the shielding absorbing particles and shielding absorbing particles.
Preferably, the volume ratio of the high molecular polymer, the shielding wave-absorbing particles and the foaming powder in the embodiment of the application is 1:1:1. Under the proportion, the effect of the high polymer adhesive can be fully exerted, the synergistic effect of the shielding wave-absorbing particles and the foaming powder can be maximized, and the electromagnetic shielding effect is improved.
Step 22, continuously laying the carbon nano tube continuous network aggregate with the width not more than 100mm after adding the mixed powder on the surface of a rotary metal (usually stainless steel or aluminum alloy with smooth surface and roughness less than 3.2) through multi-layer arrangement stacking, and uniformly laying the carbon nano tube continuous network aggregate on the surface of the rotary metal by utilizing the movement of the rotary metal perpendicular to the collecting direction of the carbon nano tube continuous network aggregate;
step 23, cutting the non-dense carbon nano tube continuous network aggregate membrane material containing the mixed powder uniformly laid on the surface of the roller along the axial direction of the roller, and taking down the non-dense carbon nano tube continuous network aggregate membrane material to obtain a rectangular non-dense carbon nano tube continuous network aggregate membrane material;
and step 24, performing preliminary densification treatment on the membrane material by a rolling method to ensure that the mixed powder is firmly fixed inside the carbon nano tube continuous network structure.
Step 3, after combining one or more layers of membrane materials together, placing the membrane materials in an environment with the temperature of more than 100 ℃ to melt a high polymer, and expanding and foaming powder to form hollow microspheres to obtain the porous structure shielding wave-absorbing composite material, wherein the method specifically comprises the following steps of:
after the single-layer or multi-layer film materials are combined together, the film materials are placed in a high-temperature environment with the temperature of more than 100 ℃ so as to melt the high-molecular polymer in the film materials and expand the foaming powder. The temperature can be 101 ℃, 110 ℃, 115 ℃ or 120 ℃.
In order to further shape the composite membrane and ensure the thickness consistency, a limiting plate is respectively added on the upper part and the lower part of the composite membrane to finally obtain the light electromagnetic shielding wave-absorbing composite material which has a carbon nano tube continuous network structure, high molecular polymers uniformly distributed in the composite membrane, shielding wave-absorbing particles with high-efficiency shielding effect and foaming hollow microspheres.
The second aspect of the application provides a porous structure shielding wave-absorbing composite material prepared by the preparation method of the porous structure shielding wave-absorbing composite material.
The thickness of the porous structure shielding wave-absorbing composite material obtained by the embodiment of the application is 2-4mm, and can be specifically 2mm, 2.5mm, 3mm or 4mm; density of 1.5g/cm 3 -2g/cm 3 Specifically, it may be 1.5g/cm 3 、1.7g/cm 3 、1.9g/cm 3 Or 2g/cm 3 . Within the thickness and density range, it can ensure shielding effectAnd meanwhile, the cost is reduced.
The present application will be described in more specific examples.
Example 1
Mixing epoxy resin with particle size not more than 30 μm, ferrite and sodium bicarbonate foaming agent according to a volume ratio of 1:1:1, uniformly scattering the mixture inside the non-compact carbon nano tube aggregate, rolling to obtain a composite material film with thickness of 0.2mm, placing 5 layers of the film between molds with spacing of 2mm, and then placing the films in a vacuum heat treatment furnace at 150 ℃ to obtain a composite material plate with thickness of 2 mm. The electromagnetic shielding performance test is carried out by adopting a waveguide method, and the comprehensive electromagnetic shielding efficiency is above 60dB in the wave band of 2-18GHZ, as shown in figure 2; the density of the composite board is only 1.5g/cm 3 And has better flexibility and strength, thus showing very excellent comprehensive performance.
Example 2
Polyimide, ferrite and sodium dodecyl sulfate with the particle size of more than 35 mu m are mixed according to the volume ratio of 1:1:1, uniformly scattered inside a non-compact carbon nano tube aggregate, then a composite material film with the thickness of 0.4mm is obtained through rolling, 5 layers of the film are placed between moulds with the interval of 3mm, and then the film is placed in a vacuum heat treatment furnace at the temperature of 150 ℃ to obtain a composite material plate with the thickness of 3 mm. The electromagnetic shielding performance test is carried out by adopting a waveguide method, and the comprehensive electromagnetic shielding efficiency is above 55dB in the wave band of 2-18 GHZ; the density of the composite board is only 1.8g/cm 3 And has better flexibility and strength, thus showing very excellent comprehensive performance.
Example 3
Mixing epoxy resin with particle size not more than 25 μm, ferrite and sodium bicarbonate foaming agent according to a volume ratio of 1:1:1, uniformly scattering the mixture inside the non-compact carbon nano tube aggregate, rolling to obtain a composite material film with thickness of 0.3mm, placing 5 layers of the film between molds with a spacing of 4mm, and then placing the film in a vacuum heat treatment furnace at 150 ℃ to obtain a composite material plate with thickness of 4 mm. The electromagnetic shielding performance test is carried out by adopting a waveguide method, and the comprehensive electromagnetic shielding efficiency is above 58dB in the wave band of 2-18GHZThe method comprises the steps of carrying out a first treatment on the surface of the The density of the composite board is only 2g/cm 3 And has better flexibility and strength, thus showing very excellent comprehensive performance.
The preparation method provided by the application is simple, easy to operate and low in cost, and the prepared porous structure shielding wave-absorbing composite material keeps the continuous network structure of the carbon nano tube, so that the electrical conductivity, the electromagnetic shielding effect and the stability are better.
While the application has been described in terms of preferred embodiments, it will be understood by those skilled in the art that various changes and modifications can be made without departing from the scope of the application, and it is intended that the application is not limited to the specific embodiments disclosed.
Claims (8)
1. The preparation method of the porous structure shielding wave-absorbing composite material is characterized by comprising the following steps of:
preparing a non-dense carbon nano tube continuous network aggregate;
adopting an automatic or non-automatic vibrating screen powder scattering device to scatter mixed powder into a non-compact carbon nano tube continuous network aggregate, and then rolling to obtain a membrane material; the mixed powder comprises a high molecular polymer, shielding wave-absorbing particles and foaming powder;
after one or more layers of membrane materials are combined together, placing the membrane materials in an environment with the temperature being higher than 100 ℃ to enable the high molecular polymer to melt, and expanding and foaming the foaming powder to form hollow microspheres to obtain the porous structure shielding wave-absorbing composite material;
the volume of the high molecular polymer is more than 30% of the total volume of the mixed powder;
the high molecular polymer is a thermoplastic or thermosetting resin material;
the material used for shielding the wave-absorbing particles is ferrite wave-absorbing material;
the foaming powder is sodium bicarbonate foaming agent or sodium dodecyl sulfate.
2. The method for preparing the porous structure shielding wave-absorbing composite material according to claim 1, wherein the volume ratio of the high molecular polymer to the shielding wave-absorbing particles to the foaming powder is 1:1:1.
3. The method for preparing the porous structure shielding wave-absorbing composite material according to claim 1, wherein an automatic or non-automatic vibrating screen powder scattering device is adopted to scatter mixed powder into a non-dense carbon nano tube continuous network aggregate and then roll the mixed powder, and the method specifically comprises the following steps:
and uniformly scattering the mixed powder into the non-dense carbon nano tube continuous network aggregate by adopting an automatic or non-automatic vibrating screen powder scattering device, and then rolling.
4. The method for preparing the porous structure shielding wave-absorbing composite material according to claim 1, wherein after one or more layers of the membrane materials are combined together, the membrane materials are placed in an environment with a temperature of more than 100 ℃, and the method specifically comprises the following steps:
after one or more layers of the membrane materials are combined together, limiting plates are arranged on the upper surface and the lower surface of the combined membrane materials;
and placing the combined membrane material provided with the limiting plates in an environment with the temperature of more than 100 ℃.
5. The method for preparing a porous shielding wave-absorbing composite material according to claim 1, wherein the particle sizes of the high molecular polymer, the shielding wave-absorbing particles and the foaming powder in the mixed powder are micro-particle sizes or nano-particle sizes.
6. The method for preparing the porous shielding wave-absorbing composite material according to claim 1, wherein the particle sizes of the high molecular polymer, the shielding wave-absorbing particles and the foaming powder in the mixed powder are all smaller than 30 μm.
7. A porous structure shielding wave-absorbing composite material prepared by the method for preparing a porous structure shielding wave-absorbing composite material according to any one of claims 1 to 6.
8. The porous structure shielding wave-absorbing composite of claim 7, wherein the porous structure shielding wave-absorbing composite has a thickness of 2mm-4mm and a density of 1.5g/cm 3 -2g/cm 3 。
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